3-Chloropropionyl chloride → HCID 18522615, compound

Temperature

40 °C

Into a glass-made, 500-mL reaction vessel equipped with a stirrer, the 2-(2′-mercaptoethyl)-1,3-dithiolane produced in Synthesis Example 2 (100 g, 0.60 mole) was weighed, to which 3-chloropropionic acid chloride (80 g, 0.63 mole) was added dropwise at 40° C. over 15 minutes. After the contents were reacted further under stirring at 40° C. for 8 hours, toluene (200 g) was added to the reaction mixture to dissolve the same. The resulting solution was transferred into a separating funnel, in which the solution was washed three times with a 3 wt. % aqueous solution of sodium hydrogen carbonate (300 g). After the organic layer (toluene solution) was washed with purified water (300 g) until the water layer became neutral, the organic layer was taken out, and toluene was then distilled off under reduced pressure to afford 2-[2-(3-chloropropionylthio)ethyl]-1,3-dithiolane (127 g).

1. customInto a glass-made, 500-mL reaction vessel
2. customequipped with a stirrer
3. additionwas added dropwise at 40° C. over 15 minutes
4. customAfter the contents were reacted further
5. dissolutionto dissolve the same
6. customThe resulting solution was transferred into a separating funnel, in which
7. washthe solution was washed three times with a 3 wt. % aqueous solution of sodium hydrogen carbonate (300 g)
8. washAfter the organic layer (toluene solution) was washed with purified water (300 g) until the water layer
9. distillationtoluene was then distilled off under reduced pressure

ORD record

ord-1b8c7ca53d8649fc83fede49dfa9222a

Source dataset

uspto-grants-2003_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06570025B1